#------------------------------------------------------------------------------
#$Date: 2022-07-23 01:29:16 +0200 (Sat 23 de Jul de 2022) $
#$Revision: 276812 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/51/7245155.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7245155
loop_
_publ_author_name
'Tsunashima, Ryo'
'Fujikawa, Naomi'
'Shiga, Misaki'
'Miyagawa, Sayu'
'Ohno, Shiori'
'Masuya-Suzuki, Atsuko'
'Takahashi, Kiyonori'
'Nakamura, Takayoshi'
'Akutagawa, Tomoyuki'
'Nishihara, Sadafumi'
_publ_section_title
;
 Slider-crank Mechanism in a Molecular Crystal: Conversion of Linear
 Thermal Expansion of Lattice to Circular Rotation of Coordination Chain
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00768A
_journal_year                    2022
_chemical_formula_sum            'C9 H12 Co K N5 O3'
_chemical_formula_weight         336.27
_space_group_crystal_system      hexagonal
_space_group_IT_number           190
_space_group_name_Hall           'P -6c -2c'
_space_group_name_H-M_alt        'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-03-17 deposited with the CCDC.	2022-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.3782(6)
_cell_length_b                   10.3782(6)
_cell_length_c                   7.1530(4)
_cell_measurement_reflns_used    3203
_cell_measurement_temperature    187
_cell_measurement_theta_max      29.5520
_cell_measurement_theta_min      2.2360
_cell_volume                     667.21(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      187
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1259
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6158
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.480
_diffrn_reflns_theta_min         2.266
_exptl_absorpt_coefficient_mu    1.609
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_description       block
_exptl_crystal_F_000             342
_exptl_crystal_size_max          0.290
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.221
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 229 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_coef       0.016(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         670
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0295P)²+0.0191P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.871
_reflns_number_gt                593
_reflns_number_total             670
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2ce00768a2.cif
_cod_data_source_block           187k
_cod_original_cell_volume        667.21(9)
_cod_database_code               7245155
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.653
_shelx_estimated_absorpt_t_max   0.718
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x, y, -z+1/2'
'-y, x-y, -z+1/2'
'-x+y, -x, -z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, z+1/2'
'x-y, -y, z+1/2'
'-x, -x+y, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.333333 0.666667 0.250000 0.0198(3) Uani 1 6 d S T P . .
K1 K 0.000000 0.000000 0.000000 0.0278(3) Uani 1 6 d S T P . .
O1 O 0.1908(3) 0.1950(3) 0.250000 0.0413(8) Uani 1 2 d S T P . .
N1 N 0.333333 0.666667 0.5670(4) 0.0177(6) Uani 1 3 d S T P . .
N2 N 0.2822(4) 0.4542(4) 0.250000 0.0304(7) Uani 1 2 d S T P . .
C1 C 0.1876(3) 0.5525(3) 0.6430(4) 0.0276(6) Uani 1 1 d . . . . .
H1A H 0.164979 0.455145 0.598083 0.033 Uiso 1 1 calc R U . . .
H1B H 0.110602 0.571634 0.598090 0.033 Uiso 1 1 calc R U . . .
C2 C 0.2362(4) 0.3281(4) 0.250000 0.0259(8) Uani 1 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Co1 N2 120.0 3_565 2_665 ?
N2 Co1 N2 120.0 3_565 . ?
N2 Co1 N2 120.0 2_665 . ?
N2 Co1 N1 90.0 3_565 . ?
N2 Co1 N1 90.0 2_665 . ?
N2 Co1 N1 90.0 . . ?
N2 Co1 N1 90.0 3_565 4 ?
N2 Co1 N1 90.000(1) 2_665 4 ?
N2 Co1 N1 90.0 . 4 ?
N1 Co1 N1 180.0 . 4 ?
O1 K1 O1 134.71(13) . 9 ?
O1 K1 O1 137.71(14) . 8 ?
O1 K1 O1 80.48(6) 9 8 ?
O1 K1 O1 83.55(8) . 7 ?
O1 K1 O1 80.48(6) 9 7 ?
O1 K1 O1 80.48(6) 8 7 ?
O1 K1 O1 80.48(6) . 2 ?
O1 K1 O1 83.55(8) 9 2 ?
O1 K1 O1 134.71(13) 8 2 ?
O1 K1 O1 137.71(14) 7 2 ?
O1 K1 O1 80.48(6) . 3 ?
O1 K1 O1 137.71(14) 9 3 ?
O1 K1 O1 83.55(8) 8 3 ?
O1 K1 O1 134.71(13) 7 3 ?
O1 K1 O1 80.48(6) 2 3 ?
O1 K1 C2 16.34(7) . . ?
O1 K1 C2 118.95(8) 9 . ?
O1 K1 C2 143.75(9) 8 . ?
O1 K1 C2 73.86(5) 7 . ?
O1 K1 C2 80.36(8) 2 . ?
O1 K1 C2 96.58(7) 3 . ?
O1 K1 C2 143.75(9) . 8 ?
O1 K1 C2 80.36(8) 9 8 ?
O1 K1 C2 16.34(7) 8 8 ?
O1 K1 C2 96.58(7) 7 8 ?
O1 K1 C2 118.95(8) 2 8 ?
O1 K1 C2 73.86(5) 3 8 ?
C2 K1 C2 155.49(13) . 8 ?
O1 K1 C2 118.95(8) . 9 ?
O1 K1 C2 16.34(7) 9 9 ?
O1 K1 C2 96.58(7) 8 9 ?
O1 K1 C2 80.36(8) 7 9 ?
O1 K1 C2 73.86(5) 2 9 ?
O1 K1 C2 143.75(9) 3 9 ?
C2 K1 C2 103.74(12) . 9 ?
C2 K1 C2 96.59(4) 8 9 ?
O1 K1 C2 73.86(5) . 7 ?
O1 K1 C2 96.58(7) 9 7 ?
O1 K1 C2 80.36(8) 8 7 ?
O1 K1 C2 16.34(7) 7 7 ?
O1 K1 C2 143.75(9) 2 7 ?
O1 K1 C2 118.95(8) 3 7 ?
C2 K1 C2 67.85(8) . 7 ?
C2 K1 C2 96.59(4) 8 7 ?
C2 K1 C2 96.59(4) 9 7 ?
O1 K1 C2 96.58(7) . 2 ?
O1 K1 C2 73.86(5) 9 2 ?
O1 K1 C2 118.95(8) 8 2 ?
O1 K1 C2 143.75(9) 7 2 ?
O1 K1 C2 16.34(7) 2 2 ?
O1 K1 C2 80.36(8) 3 2 ?
C2 K1 C2 96.59(4) . 2 ?
C2 K1 C2 103.74(12) 8 2 ?
C2 K1 C2 67.85(8) 9 2 ?
C2 K1 C2 155.49(13) 7 2 ?
O1 K1 C2 80.36(8) . 3 ?
O1 K1 C2 143.75(9) 9 3 ?
O1 K1 C2 73.86(5) 8 3 ?
O1 K1 C2 118.95(8) 7 3 ?
O1 K1 C2 96.58(7) 2 3 ?
O1 K1 C2 16.34(7) 3 3 ?
C2 K1 C2 96.59(4) . 3 ?
C2 K1 C2 67.85(8) 8 3 ?
C2 K1 C2 155.49(13) 9 3 ?
C2 K1 C2 103.74(12) 7 3 ?
C2 K1 C2 96.59(4) 2 3 ?
C2 O1 K1 125.25(17) . . ?
C2 O1 K1 125.25(17) . 4 ?
K1 O1 K1 83.52(8) . 4 ?
C1 N1 C1 107.34(16) 3_565 . ?
C1 N1 C1 107.34(16) 3_565 2_665 ?
C1 N1 C1 107.34(16) . 2_665 ?
C1 N1 Co1 111.53(15) 3_565 . ?
C1 N1 Co1 111.52(15) . . ?
C1 N1 Co1 111.52(15) 2_665 . ?
C2 N2 Co1 172.3(3) . . ?
N1 C1 C1 111.52(15) . 4_556 ?
N1 C1 H1A 109.3 . . ?
C1 C1 H1A 109.3 4_556 . ?
N1 C1 H1B 109.3 . . ?
C1 C1 H1B 109.3 4_556 . ?
H1A C1 H1B 108.0 . . ?
N2 C2 O1 178.5(5) . . ?
N2 C2 K1 142.43(17) . . ?
O1 C2 K1 38.41(13) . . ?
N2 C2 K1 142.43(17) . 4 ?
O1 C2 K1 38.41(13) . 4 ?
K1 C2 K1 60.89(6) . 4 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N2 1.993(3) 3_565 ?
Co1 N2 1.993(3) 2_665 ?
Co1 N2 1.993(3) . ?
Co1 N1 2.267(3) . ?
Co1 N1 2.267(3) 4 ?
K1 O1 2.685(2) . ?
K1 O1 2.685(2) 9 ?
K1 O1 2.685(2) 8 ?
K1 O1 2.685(2) 7 ?
K1 O1 2.685(2) 2 ?
K1 O1 2.685(2) 3 ?
K1 C2 3.529(3) . ?
K1 C2 3.529(3) 8 ?
K1 C2 3.529(3) 9 ?
K1 C2 3.529(3) 7 ?
K1 C2 3.529(3) 2 ?
K1 C2 3.529(3) 3 ?
O1 C2 1.216(4) . ?
N1 C1 1.481(3) 3_565 ?
N1 C1 1.481(3) . ?
N1 C1 1.481(3) 2_665 ?
N2 C2 1.147(5) . ?
C1 C1 1.531(5) 4_556 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C1 C1 -57.57(17) 3_565 . . 4_556 ?
C1 N1 C1 C1 57.56(17) 2_665 . . 4_556 ?
Co1 N1 C1 C1 179.998(0) . . . 4_556 ?
K1 O1 C2 K1 -109.3(4) 4 . . . ?
K1 O1 C2 K1 109.3(4) . . . 4 ?
